CN111019454B - Ultrathin water-based intumescent steel structure nano flame-retardant coating and preparation method thereof - Google Patents
Ultrathin water-based intumescent steel structure nano flame-retardant coating and preparation method thereof Download PDFInfo
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
- C09D5/185—Intumescent paints
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K2003/2237—Oxides; Hydroxides of metals of titanium
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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Abstract
The invention provides an ultrathin water-based intumescent steel structure nano flame-retardant coating and a preparation method thereof, belonging to the technical field of flame-retardant materials. The traditional ammonium polyphosphate-melamine-pentaerythritol is used as an expansion flame-retardant system, the peptide dioxide is used as a filler, and an inorganic nano flame-retardant compound containing nano aluminum hydroxide, graphene and nano silicon dioxide is added to prepare the ultrathin aqueous expansion type steel structure nano flame-retardant coating. In the preparation process, graphene and nano-silica are firstly mixed to form a stable nano-silica-graphene system, then nano-aluminum hydroxide is added to form a weak chemical bond of Al-O-Si, and meanwhile, membrane contact mixing is adopted to improve the dispersity of the nano-material, improve the hydrophobic property of the flame retardant coating and improve the adhesive force of the flame retardant coating and a base material.
Description
Technical Field
The invention belongs to the technical field of flame retardant materials, and particularly relates to an ultrathin water-based intumescent steel structure nano flame retardant coating and a preparation method thereof.
Background
The steel structure is used as the main form of modern buildings, and has the advantages of light weight, high strength, good earthquake resistance, short construction period, high building industrialization degree, high space utilization rate, investment saving and the like. The critical temperature of the mechanical property of the steel is 540 ℃, when a building is in fire, the temperature of a fire scene can reach about 1000 ℃ within a few minutes, the bare steel can quickly rise to the critical temperature of more than 540 ℃, the bearing capacity of the bare steel can be rapidly reduced to cause the collapse of the building, and therefore huge property loss and serious casualties are caused. Therefore, fire protection of steel structures is necessary, and the use of fire-retardant coatings is an ideal protection method.
At present, the fire-proof paint for the ultra-thin steel structure is widely applied to the domestic steel structure fire protection, and is an expansion type paint, and the using amount of the paint almost accounts for 90 percent of the total fire-proof paint. The expansion type steel structure fire-proof coating is made up by using natural or synthetic high polymer (generally resin or emulsion) as base material, adding dewatering carbon-forming catalyst, carbon-forming agent and foaming agent, adding the mixture of inorganic flavouring material and adjuvant, at normal temp. forming coating layer whose thickness is 1.5 mm-3 mm, when fire disaster occurs, it can be expanded and carbonized to form 40 mm-100 mm carbonized layer, so that it can play the role of fire-proofing protection. The common water-based fireproof flame-retardant coating has a plurality of defects, which are mainly shown in that the fireproof performance is poor, the strength of the coating is poor after the coating expands in case of fire, the coating can be peeled off, the fireproof performance is influenced, the durability and the aging resistance are poor, the binding force between the coating and a base material can be gradually reduced, the fireproof performance is influenced, and the smoke safety problem exists in case of fire.
Research shows that the nanometer material has quantum size effect, surface effect, macroscopic quantum tunneling effect and lotus leaf amphiphobic characteristic, so that when the nanometer material is applied to the fireproof coating, the fireproof limit, bonding strength, adhesive force, waterproofness, weather resistance and color and luster of the fireproof coating can be obviously improved, however, the nanometer material cannot be well dispersed in a solvent system of the coating due to the self-agglomeration property, so that the fireproof performance of the nanometer fireproof coating is limited.
In the prior art, some nano-type fire-retardant coatings and preparation methods thereof are provided, which modify nano-materials, such as nano-silica, nano-aluminum hydroxide, nano-magnesium hydroxide, nano-montmorillonite, and the like, for example, coupling and grafting are performed by using coupling agents, modifiers, and the like, so as to improve the dispersibility of the nano-materials. However, the surface property of the nano material is changed regardless of the use of the coupling agent or the modifying agent, so that the surface migration capacity of the fireproof coating is enhanced, the fire endurance of the nano fireproof coating and the adhesive force and the adhesive strength when the nano fireproof coating is combined with a base material are reduced, the coating thickness of the fireproof coating is increased to a certain extent, and the application of the nano fireproof coating is limited.
Disclosure of Invention
In view of the above, there is a need to provide an ultrathin aqueous intumescent steel structure nano flame retardant coating and a preparation method thereof, so as to solve the technical problems existing in the prior art that after a nano material is modified, the surface performance of the nano material is reduced, and the fire endurance of the nano type fireproof coating and the adhesion and bonding strength when the nano type fireproof coating is combined with a base material are reduced.
An ultrathin water-based intumescent steel structure nano flame-retardant coating comprises the following materials in parts by weight:
15-45 parts of a film forming agent; 10-15 parts of ammonium polyphosphate; 10-20 parts of pentaerythritol; 15-25 parts of melamine; 8-20 parts of nano titanium dioxide filler; 0.15-1 part of assistant; 5-25 parts of inorganic nano flame-retardant compound and 10-30 parts of water;
wherein the inorganic nano flame-retardant compound comprises nano aluminum hydroxide, graphene and nano silicon dioxide in a weight ratio of (1-3) to 1.
In one embodiment, the material comprises the following materials in parts by weight:
15-45 parts of a film forming agent; 10-15 parts of ammonium polyphosphate; 10-20 parts of pentaerythritol; 15-25 parts of melamine; 8-20 parts of nano titanium dioxide filler; 0.15-1 part of assistant; 15-25 parts of inorganic nano flame-retardant compound and 10-30 parts of water;
the inorganic nano flame-retardant compound comprises nano aluminum hydroxide, graphene and nano silicon dioxide in a weight ratio of 2:2: 1.
The preparation method of the ultrathin water-based intumescent steel structure nano flame retardant coating comprises the following steps:
a. preparing an inorganic nano flame-retardant compound:
a1. weighing graphene and nano silicon dioxide according to the weight ratio of (1-3): 1, and fully mixing the graphene and the silicon dioxide in a high-temperature environment to prepare an inorganic mixture A;
a2. weighing nano aluminum hydroxide with the weight equal to that of the graphene, adding the nano aluminum hydroxide into the inorganic mixture A under a high-temperature environment, and fully mixing the nano aluminum hydroxide and the inorganic mixture A to prepare an inorganic nano flame-retardant compound;
b. preparation of ultrathin water-based expansion type steel structure nano flame-retardant coating
b1. 10-15 parts of ammonium polyphosphate by weight; 10-20 parts of pentaerythritol; 15-25 parts of melamine; 8-20 parts of nano titanium dioxide filler; 0.15 to 1 portion of auxiliary agent is fully and uniformly mixed in 10 to 30 portions of water, and slurry B is obtained after grinding;
b2. filming the slurry B on the wall of the contact mixer to form a slurry film C;
b3. according to the weight, 5 to 25 parts of inorganic nano flame-retardant compound is contacted with the C slurry film at the speed of 0.2 to 0.5 parts/min to obtain D mixed solution;
b4. and fully stirring the mixed solution D, adding 15-45 parts of film forming agent into the mixed solution, and mixing at a high speed to prepare the ultrathin water-based intumescent steel structure nano flame retardant coating.
In one embodiment, the film forming agent comprises at least one of silicone resin, acrylic resin, amino resin, vinyl ester resin, styrene-acrylic emulsion, silicone-acrylic emulsion.
In one embodiment, the high temperature environment is 100 ℃ to 150 ℃ in step a1 and step a2.
In one embodiment, the auxiliary agent comprises a water repellent agent, a leveling agent, an antifoaming agent and a flame retardant synergist in a weight ratio of 1 (0.5-0.8) to 0.1-0.5 to 1-2.
In one embodiment, the flame retardant synergist comprises at least one of vermiculite, expandable graphite and perlite.
In one embodiment, the contact mixer comprises a contact tank and a solid hourglass, the slurry B flows in from the tank wall of the contact tank and is formed on the inner wall of the contact tank, the lower end of the solid hourglass is provided with a bell-mouth-shaped feed opening, and the feed opening is close to the inner wall of the contact tank.
The method is characterized in that traditional ammonium polyphosphate (APP) -Melamine (MEL) -Pentaerythritol (PER) is used as an expansion flame-retardant system, peptide dioxide is used as a filler, and an inorganic nano flame-retardant compound containing nano aluminum hydroxide, graphene and nano silicon dioxide is added to prepare the ultrathin water-based expansion type steel structure nano flame-retardant coating, the prepared ultrathin water-based expansion type steel structure nano flame-retardant coating is excellent in performance, the Limiting Oxygen Index (LOI) reaches over 36%, the vertical combustion level can reach UL 94V-0 level, the smoke density meets the requirement that the A-level flame-retardant coating SDR specified by GB/T8627 is less than or equal to 15, the coating expands rapidly and uniformly, and a carbon layer is compact. Firstly, mixing graphene and nano silicon dioxide, enabling the nano silicon dioxide and graphene molecules to violently collide at high temperature, enabling the nano silicon dioxide to be inlaid into an interlayer structure of the graphene to form a stable nano silicon dioxide-graphene system, secondly, mixing nano aluminum hydroxide and the nano silicon dioxide-graphene system at high temperature to form weak bond connection of Al-O-Si, and further improving the adhesive force and the adhesive degree of the prepared ultrathin aqueous intumescent steel structure nano flame retardant coating and a base material.
Drawings
FIG. 1 is a schematic diagram of a contact mixer according to an embodiment.
FIG. 2 is a cross-sectional view of a contact mixer in one embodiment.
Fig. 3 is a partially enlarged view of a portion a shown in fig. 2.
In the figure: the device comprises a contact mixer 10, a contact tank 100, an inner mixing tank 110, a film-forming overflow hole 111, an outer liquid storage tank 120, a movable lifting plate 121, a solid hourglass 200, a feed opening 201, a storage cavity 210, a feed pipe 220, a feed cavity 230, a feed distributor 240, a feed valve 250 and a feed hole 251.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
It will be understood that when an element is referred to as being "disposed on" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. As used herein, the terms "vertical," "horizontal," "left," "right," "top," "bottom," "top," and the like are for illustrative purposes only and do not represent the only embodiments.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items. To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
In one embodiment, a method for preparing the ultrathin water-based intumescent steel structure nano flame retardant coating comprises the following steps:
a. preparing an inorganic nano flame-retardant compound:
a1. weighing graphene and nano silicon dioxide according to the weight ratio of (1-3): 1, and fully mixing the graphene and the silicon dioxide in a high-temperature environment to prepare an inorganic mixture A;
a2. weighing nano aluminum hydroxide with the weight equal to that of the graphene, adding the nano aluminum hydroxide into the inorganic mixture A under a high-temperature environment, and fully mixing the nano aluminum hydroxide and the inorganic mixture A to prepare an inorganic nano flame-retardant compound;
b. preparation of ultrathin water-based expansion type steel structure nano flame-retardant coating
b1. 10-15 parts of ammonium polyphosphate by weight; 10-20 parts of pentaerythritol; 15-25 parts of melamine; 8-20 parts of nano titanium dioxide filler; 0.15 to 1 portion of auxiliary agent is fully and uniformly mixed in 10 to 30 portions of water, and slurry B is obtained after grinding;
b2. filming the slurry B on the wall of the contact mixer to form a slurry film C;
b3. according to the weight, 5 to 25 parts of inorganic nano flame-retardant compound is contacted with the C slurry film at the speed of 0.2 to 0.5 parts/min to obtain D mixed solution;
b4. and fully stirring the mixed solution D, adding 15-45 parts of film forming agent into the mixed solution, and mixing at a high speed to prepare the ultrathin water-based intumescent steel structure nano flame retardant coating.
The ultrathin water-based intumescent steel structure nano flame-retardant coating prepared by the method has excellent performance, the Limiting Oxygen Index (LOI) reaches over 36 percent, the vertical combustion grade can reach UL 94V-0 level, the smoke density reaches the requirement that the A-level flame-retardant coating SDR specified by GB/T8627 is less than or equal to 15, the coating expands rapidly and uniformly, and the carbon layer is compact. Firstly, mixing graphene and nano silicon dioxide, enabling the nano silicon dioxide and graphene molecules to violently collide at high temperature, enabling the nano silicon dioxide to be inlaid into an interlayer structure of the graphene to form a stable nano silicon dioxide-graphene system, secondly, mixing nano aluminum hydroxide and the nano silicon dioxide-graphene system at high temperature to form weak bond connection of Al-O-Si, and further improving the adhesive force and the adhesive degree of the prepared ultrathin aqueous intumescent steel structure nano flame retardant coating and a base material. Secondly, in the preparation process of the ultrathin water-based intumescent steel structure nano flame-retardant coating, the inorganic nano flame-retardant composite with higher hydrophobicity and the B slurry formed by uniformly mixing the components are subjected to membrane contact mixing, and the contact mixing speed of the inorganic nano flame-retardant composite is controlled, so that the inorganic nano flame-retardant composite can be further uniformly dispersed in the B slurry system, and the problem that the nano material is directly added into the liquid phase, the nano material is agglomerated, the nano material is unevenly distributed, and the quality of the nano flame-retardant coating is reduced is avoided.
The ultra-thin water-based intumescent steel structure nano flame-retardant coating and the preparation method thereof are described below with reference to specific examples to further understand the inventive concepts of the ultra-thin water-based intumescent steel structure nano flame-retardant coating and the preparation method thereof.
In one embodiment, the preparation method of the ultrathin water-based intumescent steel structure nano flame retardant coating comprises the following steps:
s10, preparing an inorganic nano flame-retardant compound.
S11, weighing graphene and nano silicon dioxide according to the weight ratio of (1-3): 1, and fully mixing the graphene and the silicon dioxide in a high-temperature environment to prepare an inorganic mixture A. Specifically, graphene and nano silicon dioxide are weighed according to the weight ratio (1-3): 1, the mixture is placed into a heatable mixing container, the mixing container is placed into an oil bath pot, the temperature of the oil bath is controlled to be 100-150 ℃, preferably 120 ℃, the mixture is manually and slowly stirred for 30-60 min, and the nano silicon dioxide can be fully embedded into the interlayer structure of the graphene. Further, after stirring is stopped, the oil bath temperature is maintained at 100-150 ℃, and standing is kept for 10-30 min, so that a system formed by the nano silicon dioxide and the graphene is stable.
S12, weighing nano aluminum hydroxide with the weight equal to that of the graphene, adding the nano aluminum hydroxide into the inorganic mixture A under a high-temperature environment, and fully mixing the nano aluminum hydroxide and the inorganic mixture A to prepare the inorganic nano flame-retardant compound. Specifically, nano aluminum hydroxide with the weight equal to that of graphene is weighed, namely the mass ratio of the nano aluminum hydroxide to the graphene is maintained at about 1:1, the weighed nano aluminum hydroxide is added into the mixing container, the temperature of an oil bath is controlled to be 100-150 ℃, preferably 120 ℃, the nano aluminum hydroxide is manually and slowly stirred for 30-60 min, so that the nano aluminum hydroxide, the nano silicon dioxide and graphene mixed system are uniformly mixed, and the Al-O-Si weak bond connection is formed. And after the mixing is finished, stopping stirring, and slowly cooling to room temperature to obtain the inorganic nano flame-retardant compound in a mixing container.
S20, preparing the ultrathin water-based intumescent steel structure nano flame-retardant coating.
S21, according to the weight, 10-15 parts of ammonium polyphosphate are added; 10-20 parts of pentaerythritol; 15-25 parts of melamine; 8-20 parts of nano titanium dioxide filler; 0.15 to 1 portion of the auxiliary agent is fully and uniformly mixed in 10 to 30 portions of water, and the mixture is ground to obtain slurry B. Specifically, the above substances are weighed according to the weight, added into deionized water, stirred to be fully mixed to form slurry, and the obtained slurry is fully ground in a ball mill to obtain slurry B.
In the above process, the weight of each substance is not strictly limited, and for example, 12 parts of ammonium polyphosphate, 15 parts of pentaerythritol, 15 parts of melamine, 10 parts of nano titanium dioxide filler and 1 part of auxiliary agent are fully mixed in 30 parts of water. Preferably, the viscosity of the obtained B slurry is configured to be 8pa · s to 15pa · s, so that the obtained B slurry has good fluidity and strong viscosity.
For example, the auxiliary agent comprises a water repellent agent, a leveling agent, an antifoaming agent and a flame retardant synergist in a weight ratio of 1 (0.5-0.8) to 0.1-0.5 (1-2). Preferably, the weight ratio of the water repellent agent, the leveling agent, the defoaming agent and the flame retardant synergist is 1:0.5:0.1: 2.
For example, the flame retardant synergist comprises at least one of vermiculite, expandable graphite and perlite, and preferably, the flame retardant synergist is expandable graphite so as to further promote the thin water-based expansion type steel structure nano flame retardant coating to form a compact carbonized layer after encountering high temperature.
S22, the slurry B is filmed on the wall of the contact mixer to form a slurry C film, even if the obtained slurry B flows down along the inner wall of the contact mixer, at the moment, the slurry B forms a layer of uniformly distributed liquid film on the wall of the contact mixer, namely the slurry C film, and the thickness of the slurry C film can be controlled according to the feeding speed of the slurry B.
S23, contacting 5-25 parts by weight of inorganic nano flame-retardant compound with the C slurry film at the speed of 0.2-0.5 part/min to obtain D mixed solution.
Referring to fig. 1 to 3, in order to facilitate the membrane contact mixing process adopted in the present invention, in one embodiment, a contact mixer 10 is provided, the contact mixer 10 includes a contact tank 100 and a solid hourglass 200, a B slurry flows in from the tank wall of the contact tank 100 and is formed on the inner wall of the contact tank 100, the lower end of the solid hourglass 200 is provided with a bell-mouth-shaped feed opening 201, and the feed opening is close to the inner wall of the contact tank 100. The inorganic nano flame-retardant compound uniformly flows down from the feed opening 201 of the solid hourglass 200, is in contact with a liquid film formed on the inner wall of the contact tank 100, and falls into the bottom of the contact tank 100 along with the slurry B. And a stirring paddle is arranged at the bottom of the contact tank, and the slurry B mixed with the inorganic nano flame-retardant compound at the bottom of the contact tank is fully stirred, so that the inorganic nano flame-retardant compound is fully dispersed in the slurry B.
Specifically, the contact tank 100 includes an inner mixing tank 110 and an outer liquid storage tank 120, the outer liquid storage tank 120 is sleeved outside the inner mixing tank 110, and a liquid storage cavity for containing B slurry is formed between an inner tank wall of the outer liquid storage tank 120 and an outer tank wall of the inner mixing tank 110. The upper end of the wall of the inner mixing tank 110, which is close to the inner mixing tank 110, is provided with a film-forming overflow hole 111, the outer liquid storage tank 120 is provided with a movable lifting plate 121, the movable lifting plate 121 is in contact with and sealed with the outer wall of the inner mixing tank 110 and the inner wall of the outer liquid storage tank 120, and the movable lifting plate 121 can slide up and down along the liquid storage cavity. When the movable lifting plate 121 is located at the lowest point, the prepared B slurry is added into the liquid storage cavity, the movable lifting plate 121 is slowly lifted upwards, the liquid level of the B slurry rises, and overflows from the film forming overflow hole 111 into the mixing inner groove 110, and a uniform liquid film is formed on the inner groove wall of the mixing inner groove 110. A handle may be disposed at the upper end of the movable lifting plate 121 to manually control the lifting speed of the movable lifting plate 121, or a lifting cylinder may be disposed at the bottom of the movable lifting plate 121 to automatically control the lifting speed of the movable lifting plate 121, so that the movable lifting plate 121 rises at a constant speed, and the uniform thickness of the formed film is ensured.
Further, in order to ensure that the inorganic nano flame-retardant compound can be uniformly sprinkled on the liquid film on the inner wall of the inner mixing tank 110, the solid-phase hourglass 200 comprises a storage cavity 210, a discharging pipe 220 and a discharging cavity 230, wherein the bottom of the discharging cavity 210 is reduced in diameter and is connected with the discharging pipe 220, the upper part of the discharging cavity 230 is reduced in diameter and is connected with the discharging pipe 220, a conical discharging distributor 240 is arranged in the discharging cavity 230, and the fixed point of the discharging distributor 240 is close to the lower end of the discharging pipe 220 and is located at the geometric center of the lower end of the discharging pipe 220. The blanking distributor 240 and a material dispersing cavity is formed between the cavity walls of the blanking cavity 230, the bottom of the material dispersing cavity is provided with the blanking opening 201, the discharging direction of the blanking opening 201 is tangent to the lower end of the blanking cavity 230, and the blanking opening 201 is close to the inner wall of the inner mixing groove 110.
The weighed inorganic nano flame-retardant compound is poured into the storage cavity 210, flows into the blanking cavity 230 from the bottom of the storage cavity 210 through the blanking pipe 220, falls along the side wall of the blanking distributor 240 under the dispersion action of the blanking distributor 240, is guided out from the blanking port 201, contacts with the liquid film on the inner wall of the inner mixing groove 110, flows to the bottom of the inner mixing groove 110 along with the liquid film, is uniformly mixed under the stirring action, and the dispersion degree of the inorganic nano flame-retardant compound is improved.
Further, in order to control the blanking amount of the inorganic nano flame-retardant composite, a blanking valve 250 is arranged on the blanking pipe 220, the blanking valve 250 is a long round rod, and the blanking valve 250 is inserted in the middle of the blanking pipe 220 and can slide left and right along the blanking pipe 220. The blanking valve is provided with a plurality of blanking holes 251 with different sizes. The blanking valve 250 is slid along a direction perpendicular to the blanking pipe 220, so that the blanking pipe is communicated with the blanking holes 251 at different positions, thereby realizing blanking at different flow rates, and controlling the blanking amount of the inorganic nano flame-retardant compound.
In one embodiment, the slurry B can be circulated, and the inorganic nano flame-retardant compound is contacted and mixed with the slurry B by a small amount of the circulated slurry B for multiple times, so that the mixing is more uniform, and the inorganic nano flame-retardant compound is more dispersed. In this case, the slurry B may be transferred back to the outer tank 120 by, for example, air compression or the like by providing a communication pipe between the inner mixing tank 110 and the outer tank 120.
S24, fully stirring the mixed solution D, adding 15-45 parts of film forming agent into the mixed solution, and mixing at a high speed to prepare the ultrathin water-based intumescent steel structure nano flame retardant coating.
For example, the film forming agent includes at least one of silicone resin, acrylic resin, amino resin, vinyl ester resin, styrene-acrylic emulsion, and silicone-acrylic emulsion. Preferably, the film forming agent is acrylic resin or a mixture of acrylic resin and organic silicon resin, so as to improve the film forming property of the thin water-based intumescent steel structure nano flame retardant coating.
The technical solutions and the technical effects thereof according to the present invention are further described below by specific examples.
Examples 1 to 6
Weighing and preparing the materials according to the weight ratio of the materials shown in the following table, and preparing the ultrathin water-based intumescent steel structure nano flame-retardant coating by adopting the method of the specific embodiment, wherein the temperature of mixing the graphene and the nano silicon dioxide is 150 ℃, the stirring is carried out for 30min, the stay time is 30min, the temperature of mixing the nano aluminum hydroxide is 150 ℃, and the stirring is carried out for 30 min. Wherein the inorganic nano flame retardant composite is circularly mixed with the B slurry at a rate of 0.2 parts/min.
TABLE materials configuration List for examples 1-6
Examples 1-6 the same other components were maintained, and the properties of 6 ultrathin aqueous intumescent steel structure nano flame retardant coatings prepared by changing the parts by weight of nano aluminum hydroxide, graphene and nano silica under the same process conditions were tested by the national standard method, as shown in the table below.
TABLE II Table 1-6 Table for evaluating the performance of the ultra-thin water-based intumescent steel structure nano flame retardant coating prepared
From the above table, the ultrathin water-based intumescent steel structure nano flame retardant coating prepared by the method provided by the invention has excellent performance, and especially shows excellent performance in cold and heat cycle resistance, water resistance, adhesion and the like.
Examples 7 to 12
Weighing and preparing the materials according to the weight ratio of the materials shown in the following table, and preparing the ultrathin water-based intumescent steel structure nano flame-retardant coating by adopting the method of the specific embodiment, wherein the temperature of mixing the graphene and the nano silicon dioxide is 100 ℃, the stirring is carried out for 60min, the stay time is 10min, the temperature of mixing the nano aluminum hydroxide is 100 ℃, and the stirring is carried out for 60 min. Wherein the inorganic nano flame retardant composite is circularly mixed with the B slurry at a rate of 0.5 parts/min.
Table iii materials list for examples 7-12
Examples 1-6 keep the same weight parts of nano aluminum hydroxide, graphene and nano silicon dioxide, change the ratios of different film forming agents, flame retardant system substances, fillers and auxiliaries, and test the properties of 6 ultrathin aqueous intumescent steel structure nano flame retardant coatings prepared by the same process conditions by adopting a national standard method, as shown in the following table.
TABLE IV evaluation table for performance of ultra-thin water-based intumescent steel structure nano flame retardant coating prepared in examples 7-12
From the above table, the ultrathin water-based intumescent steel structure nano flame retardant coating prepared by the method provided by the invention has excellent performance, and especially shows excellent performance in cold and heat cycle resistance, water resistance, adhesion and the like.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (6)
1. A preparation method of ultrathin water-based intumescent steel structure nano flame retardant coating is characterized by comprising the following steps:
a. preparing an inorganic nano flame-retardant compound:
a1. weighing graphene and nano silicon dioxide according to the weight ratio of (1-3): 1, and fully mixing the graphene and the silicon dioxide in a high-temperature environment to prepare an inorganic mixture A;
a2. weighing nano aluminum hydroxide with the weight equal to that of the graphene, adding the nano aluminum hydroxide into the inorganic mixture A under a high-temperature environment, and fully mixing the nano aluminum hydroxide and the inorganic mixture A to prepare an inorganic nano flame-retardant compound;
b. the preparation of the ultrathin water-based intumescent steel structure nano flame retardant coating comprises the following steps:
b1. 10-15 parts of ammonium polyphosphate by weight; 10-20 parts of pentaerythritol; 15-25 parts of melamine; 8-20 parts of nano titanium dioxide filler; 0.15 to 1 portion of auxiliary agent is fully and uniformly mixed in 10 to 30 portions of water, and slurry B is obtained after grinding;
b2. filming the slurry B on the wall of the contact mixer to form a slurry film C; the contact mixer comprises a contact groove and a solid-phase hourglass, slurry B flows in from the groove wall of the contact groove and forms a film on the inner wall of the contact groove, the lower end of the solid-phase hourglass is provided with a bell-mouth-shaped feed opening, and the feed opening is close to the inner wall of the contact groove;
b3. according to the weight, 5 to 25 parts of inorganic nano flame-retardant compound is contacted with the C slurry film at the speed of 0.2 to 0.5 parts/min to obtain D mixed solution;
b4. and fully stirring the mixed solution D, adding 15-45 parts of film forming agent into the mixed solution, and mixing at a high speed to prepare the ultrathin water-based intumescent steel structure nano flame retardant coating.
2. The method for preparing the ultrathin aqueous intumescent steel structure nano flame retardant coating as claimed in claim 1, wherein the film forming agent comprises at least one of silicone resin, amino resin, vinyl ester resin, styrene-acrylic emulsion, silicone-acrylic emulsion.
3. The method for preparing the ultrathin aqueous intumescent steel structure nano flame retardant coating as claimed in claim 1, wherein the high temperature environment in step a1 and step a2 is 100 ℃ to 150 ℃.
4. The method for preparing the ultrathin aqueous intumescent steel structure nano flame retardant coating as claimed in claim 1, wherein the auxiliary comprises a water repellent agent, a leveling agent, a defoaming agent and a flame retardant synergist in a weight ratio of 1 (0.5-0.8) to (0.1-0.5) to (1-2).
5. The method for preparing the ultrathin aqueous intumescent steel structure nano flame retardant coating as claimed in claim 4, wherein the flame retardant synergist comprises at least one of vermiculite, expandable graphite and perlite.
6. An ultrathin aqueous intumescent steel structure nano flame-retardant coating, which is characterized by being prepared by the preparation method of the ultrathin aqueous intumescent steel structure nano flame-retardant coating as claimed in any one of claims 1 to 5.
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WO1994017142A1 (en) * | 1993-01-22 | 1994-08-04 | Minnesota Mining And Manufacturing Company | Intumescent fire protection coatings |
CN104327619A (en) * | 2014-11-05 | 2015-02-04 | 北京化工大学 | Water-based intumescent profiled steel structure fire-resistant paint and preparation method thereof |
CN106085220A (en) * | 2016-05-13 | 2016-11-09 | 杭州师范大学 | A kind of preparation method and applications of organic silicon flame-retardant fireproof coating |
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